Water → 2,3-Diaminobenzoic acid

HRID 380516

反応式

HRID 380516 の反応式
[N+:1]([C:4]1[C:12]([N+:13]([O-])=O)=[CH:11][CH:10]=[CH:9][C:5]=1[C:6]([OH:8])=[O:7])([O-])=O.Cl[Sn]Cl.O>C(O)(=O)C.Cl>[NH2:1][C:4]1[C:12]([NH2:13])=[CH:11][CH:10]=[CH:9][C:5]=1[C:6]([OH:8])=[O:7]

参加物

6

反応物 3

HCID 962WaterHCID 24479Stannous ChlorideHCID 2833272,3-Dinitrobenzoic acid

生成物 1

HCID 1980692,3-Diaminobenzoic acid収率 97.9%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 313Hydrochloric Acid溶媒

実験手順

To a suspension of 2 g (9.4 mmol) of 2,3-di-nitrobenzoic acid in 20 mL of acetic acid at 0° C. was added a solution of 14.8 g (65 mmol) SnCl2. 2 H2O in 7 mL of concentrated HCl. After stirring for 2 h at rt, the reaction mixture was concentrated. The residue was dissolved in 30 mL of H2O and the pH was adjusted to pH=12-13 with 6N NaOH. The mixture was filtered and the solid was washed with 0.1N HCl. The combined aqueous fractions were concentrated to give 1.4 g of the title compound.

後処理

  1. concentrationthe reaction mixture was concentrated
  2. dissolutionThe residue was dissolved in 30 mL of H2O
  3. filtrationThe mixture was filtered
  4. washthe solid was washed with 0.1N HCl
  5. concentrationThe combined aqueous fractions were concentrated

出典と根拠

ORDレコード
ord-894b9a44de43464aad84271e1e113347
出典データセット
uspto-grants-2001_10
特許番号
US06303593B1

関連ノート

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